Agilent 1200 Series Variable Wavelength Detector G1314B /G1314C (SL) User Manual A
Notices © Agilent Technologies, Inc. 2006 Warranty No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws. The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions.
In This Manual… This manual covers the Agilent 1200 Series Variable Wavelength Detectors 1 G1314B Agilent 1200 Series VWD G1314C Agilent 1200 Series VWD-SL Introduction to the Variable Wavelength Detector This chapter gives an introduction to the detector, instrument overview and internal connectors. 2 Site Requirements and Specifications This chapter gives information on environmental requirements, physical and performance specifications.
9 Parts and Materials for Maintenance This chapter provides information on parts for maintenance. A Appendix This chapter provides addition information on safety, legal and web.
Contents 1 Introduction to the Variable Wavelength Detector Introduction to the Detector Optical System Overview Electrical Connections Instrument Layout 10 11 15 17 Early Maintenance Feedback (EMF) EMF Counter 18 Using the EMF Counters 18 2 Site Requirements and Specifications Site Requirements 22 Physical Specifications 24 Performance Specifications 3 25 Installing the Detector Unpacking the Detector 28 Optimizing the Stack Configuration Installing the Detector 30 33 Flow Connections to t
Optimization of the System 44 Preparing the HPLC System 45 Running the Sample and Verifying the Results 54 Special Settings of the Detector 55 Control Settings 55 Online Spectra 56 Scanning with the VWD 57 Analog Output Settings 59 Special Setpoints 60 Peakwidth Settings 61 Optimizing the Detector 63 5 How to optimize the detector Optimizing the Detector Performance 66 Match the Flow Cell to the Column 66 Set the Detector Parameters 69 6 Troubleshooting and Diagnostics Overview of the Detector’s Indica
Cleaning the Detector 80 Using the ESD Strap 8 81 Maintenance Overview of Maintenance Exchanging a Lamp 84 85 Exchanging a Flow Cell 87 Repairing the Flow Cells 90 Using the Cuvette Holder Correcting Leaks 94 97 Replacing Leak Handling System Parts Replacing the Interface Board 99 Replacing the Detector’s Firmware Tests & Calibrations Intensity Test 100 101 102 Wavelength Verification/Calibration Holmium Oxide Test 9 98 104 105 Parts and Materials for Maintenance Overview of Maintena
Accessory Kit A 118 Appendix General Safety Information 120 Lithium Batteries Information Radio Interference Sound Emission UV-Radiation 123 124 125 126 Solvent Information 127 Declaration of Conformity for HOX2 Filter Agilent Technologies on Internet 129 130 Index 8 1200 Series Variable Wavelength Detector User Manual
Agilent 1200 Series Variable Wavelength Detector User Manual 1 Introduction to the Variable Wavelength Detector Introduction to the Detector 10 Optical System Overview 11 Flow Cell 12 Electrical Connections 15 Instrument Layout 17 Early Maintenance Feedback (EMF) 18 This chapter gives an introduction to the detector, instrument overview and internal connectors.
1 Introduction to the Variable Wavelength Detector Introduction to the Detector The Agilent 1200 Series variable wavelength detector is designed for highest optical performance, GLP compliance and easy maintenance with: • higher data rate (27/55Hz) for fast-HPLC with G1314C VWD-SL, see “Set the Detector Parameters" on page 69, • deuterium lamp for highest intensity and lowest detection limit over a wavelength range of 190 to 600 nm, • optional flow-cell cartridges (standard 10 mm 14 µl, high pressure 10
Introduction to the Variable Wavelength Detector 1 Optical System Overview The optical system of the detector is shown in Figure 1. Its radiation source is a deuterium-arc discharge lamp for the ultraviolet (UV) wavelength range from 190 to 600 nm.
1 Introduction to the Variable Wavelength Detector Flow Cell A variety of flow-cell cartridges can be inserted using the same quick and simple mounting system. Figure 2 Table 1 Cartridge Type Flow Cell Flow Cell Data STD Semi-micro High Pressure Micro Maximum pressure 40 (4) 40 (4) 400 (40) 40 (4) bar (MPa) Path length 10 (conical) 6 (conical) 10 (conical) 5 mm Volume 14 5 14 1 µl Inlet i.d. 0.17 0.17 0.17 0.1 mm Inlet length 750 750 750 555 mm Outlet i.d. 0.25 0.
Introduction to the Variable Wavelength Detector 1 Lamp The light source for the UV wavelength range is a deuterium lamp. As a result of plasma discharge in a low pressure deuterium gas, the lamp emits light over the 190 to 600 nm wavelength range. Source Lens Assembly The source lens receives the light from the deuterium lamp and focuses it onto the entrance slit. Entrance Slit Assembly The entrance slit assembly has an exchangeable slit. The standard one has a 1-mm slit.
1 Introduction to the Variable Wavelength Detector Mirror Assemblies M1 and M2 The instrument contains two spherical mirrors (M1 and M2). The beam adjustable is vertically and horizontally. Both mirrors are identical. Grating Assembly The grating separates the light beam into all its component wavelengths and reflects the light onto mirror #2. Beam Splitter Assembly The beam splitter splits the light beam. One part goes directly to the sample diode.
Introduction to the Variable Wavelength Detector 1 Electrical Connections • The GPIB connector (G1314B only) is used to connect the detector with a computer. The address and control switch module next to the GPIB connector determines the GPIB address of your detector. The switches are preset to a default address and is recognized once after power is switched ON. • The CAN bus is a serial bus with high speed data transfer.
1 Introduction to the Variable Wavelength Detector Security lever Slot for interface board Analog Signals APG Remote RS-232C serial number: DEmanufactured in Germany 62006 01week of last major change 00130number of unit CAN GPIB Power Configuration switch product number serial number safety standards configuration switch settings voltage range power consumption / frequency Figure 4 NOTE 16 Rear View of Detector - Electrical Connections and Label The G1314C VWD-SL has no GPIB connector.
Introduction to the Variable Wavelength Detector 1 Instrument Layout The industrial design of the module incorporates several innovative features. It uses Agilent’s E-PAC concept for the packaging of electronics and mechanical assemblies. This concept is based upon the use of expanded polypropylene (EPP) layers foam plastic spacers in which the mechanical and electronic boards components of the module are placed.
1 Introduction to the Variable Wavelength Detector Early Maintenance Feedback (EMF) Maintenance requires the exchange of components which are subject to wear or stress. Ideally, the frequency at which components are exchanged should be based on the intensity of usage of the instrument and the analytical conditions, and not on a predefined time interval.
Introduction to the Variable Wavelength Detector 1 counters. Enter these values (or values slightly less than the displayed values) as EMF limits, and then reset the EMF counters to zero. The next time the EMF counters exceed the new EMF limits, the EMF flag will be displayed, providing a reminder that maintenance needs to be scheduled.
1 20 Introduction to the Variable Wavelength Detector 1200 Series Variable Wavelength Detector User Manual
Agilent 1200 Series Variable Wavelength Detector User Manual 2 Site Requirements and Specifications Site Requirements 22 Physical Specifications 24 Performance Specifications 25 This chapter gives information on environmental requirements, physical and performance specifications.
2 Site Requirements and Specifications Site Requirements A suitable environment is important to ensure optimal performance of the detector. Power Consideration The detector power supply has wide ranging capabilities (see Table 2 on page 24). It accepts any line voltage in the above mentioned range. Consequently, there is no voltage selector in the rear of the detector. There are also no externally accessible fuses, because automatic electronic fuses are implemented in the power supply.
Site Requirements and Specifications WA R N I N G 2 Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations. Bench Space The detector dimensions and weight (see Table 2 on page 24) allow to place the instrument on almost any desk or laboratory bench. It needs an additional 2.5 cm (1.0 inch) of space on either side and approximately 8 cm (3.1 inches) in the rear for air circulation and electric connections.
2 Site Requirements and Specifications Physical Specifications Table 2 Physical Specifications Type Specification Weight 11 kg 25 lbs Dimensions (height × width × depth) 140 × 345 × 435 mm 5.5 × 13.
Site Requirements and Specifications 2 Performance Specifications Table 3 Performance Specifications Agilent 1200 Series Variable Wavelength Detector Type Specification Detection type Double-beam photometer Light source Deuterium lamp Wavelength range 190–600 nm Short term noise (ASTM) ± 0.75 × 10-5 AU at 254 nm See NOTE on page 26.
2 Site Requirements and Specifications Table 3 Performance Specifications Agilent 1200 Series Variable Wavelength Detector (continued) Type Specification Comments Communications Controller-area network (CAN), GPIB, RS-232C, APG Remote: ready, start, stop and shut-down signals, LAN optional GPIB for G1314B only Safety and maintenance Extensive diagnostics, error detection and display (through control module and Agilent ChemStation), leak detection, safe leak handling, leak output signal for shutdow
Agilent 1200 Series Variable Wavelength Detector User Manual 3 Installing the Detector Unpacking the Detector 28 Optimizing the Stack Configuration 30 Installing the Detector 33 Flow Connections to the Detector 36 This chapter describes the installation of the detector.
3 Installing the Detector Unpacking the Detector Damaged Packaging If the delivery packaging shows signs of external damage, please call your Agilent Technologies sales and service office immediately. Inform your service representative that the detector may have been damaged during shipment. CAUTION If there are signs of damage, please do not attempt to install the detector. Delivery Checklist Ensure all parts and materials have been delivered with the detector. The delivery checklist is shown below.
Installing the Detector 3 Detector Accessory Kit Contents Table 5 Accessory Kit Contents Description Part Number Accessory kit G1314-68705 CAN cable 0.5 m 5181-1516 1 PEEK outlet capillary kit 5062-8535 1 Fitting male PEEK 0100-1516 1 Hex key 1.
3 Installing the Detector Optimizing the Stack Configuration If your detector is part of a complete Agilent 1200 Series system, you can ensure optimum performance by installing the following configuration. This configuration optimizes the system flow path, ensuring minimum delay volume.
Installing the Detector 3 Solvent cabinet Vacuum degasser Pump Local User Interface Autosampler Column compartment Detector Figure 5 Recommended Stack Configuration (Front View) 1200 Series Variable Wavelength Detector User Manual 31
3 Installing the Detector Remote cable CAN Bus cable to local user interface CAN Bus cable Analog detector signal (1 or 2 outputs per detector) LAN to LC ChemStation (location depends on detector) Figure 6 32 Recommended Stack Configuration (Rear View) 1200 Series Variable Wavelength Detector User Manual
Installing the Detector 3 Installing the Detector Preparations Locate bench space. Provide power connections. Unpack the detector. Parts required Detector Power cord, for other cables see text below and “" on page 118 ChemStation and/or Control Module G1323B 1 Install the LAN interface board in the detector (if required), see “Replacing the Interface Board" on page 99. 2 Place the detector in the stack or on the bench in a horizontal position.
3 Installing the Detector 4 Connect the power cable to the power connector at the rear of the detector. 5 Connect the CAN cable to other Agilent 1200 Series modules. 6 If a Agilent ChemStation is the controller, connect either • the LAN connection to the LAN interface board in the detector NOTE If a Agilent 1200 DAD/MWD/FLD is in the system, the LAN should be connected to the DAD/MWD/FLD (due to higher data load). 7 Connect the analog cable (optional).
Installing the Detector 3 NOTE The detector is turned ON when the line power switch is pressed and the green indicator lamp is illuminated. The detector is turned OFF when the line power switch is protruding and the green light is OFF. WA R N I N G To disconnect the detector from line, unplug the power cord. The power supply still uses some power, even if the power switch at the front panel is turned OFF. NOTE The detector was shipped with default configuration settings.
3 Installing the Detector Flow Connections to the Detector WA R N I N G NOTE Preparations Detector is installed in the LC system.
Installing the Detector 3 3 Assemble the column-detector capillary. Depending on the flow cell type it may be a PEEK or SST capillary. 4 Connect the newly assembled fitting of the capillary to the inlet connector. 5 Connect the other end of the capillary to the column. 6 Connect the PEEK waste capillary to the outlet connector.
3 Installing the Detector 7 Establish a flow and observe for leakage. 8 Replace the front cover. The installation of the detector is now complete. NOTE 38 The detector should be operated with the front cover in place to protect the flow cell area against strong drafts from the outside.
Agilent 1200 Series Variable Wavelength Detector User Manual 4 Using the Detector Setting up an Analysis 40 Before Using the System 40 Requirements and Conditions 42 Optimization of the System 44 Preparing the HPLC System 45 Running the Sample and Verifying the Results 54 Special Settings of the Detector 55 Control Settings 55 Online Spectra 56 Scanning with the VWD 57 Analog Output Settings 59 Peakwidth Settings 61 Optimizing the Detector 63 This chapter provides information on how to set up the detector
4 Using the Detector Setting up an Analysis This chapter can be used for • preparing the system, • to learn the set up of an HPLC analysis and • to use it as an instrument check to demonstrate that all modules of the system are correctly installed and connected. It is not a test of the instrument performance. • Learn about special settings Before Using the System Solvent Information Observe recommendations on the use of solvents in chapter “Solvents” in the pump’s reference manual.
Using the Detector Table 6 4 Choice of Priming Solvents for Different Purposes Activity Solvent Comments After an installation Isopropanol Best solvent to flush air out of the system When switching between reverse phase and normal phase (both times) Isopropanol After an installation Ethanol or Methanol Best solvent to flush air out of the system To clean the system when using buffers Bidistilled water After a solvent change Alternative to Isopropanol (second choice) if no Isopropanol is avai
4 Using the Detector Requirements and Conditions What You Will Need Table 7 lists the items you need to have for the set up of the analysis. Some of these are optional (not required for the basic system). Table 7 What you will need 1200 system Pump (plus degassing) Autosampler Detector, standard flow cell installed Agilent ChemStation (B.02.01 and above) or Instant Pilot G4208 (A.01.01 and above) (optional for basic operation) or Control Module G1323B (B.04.
Using the Detector 4 Conditions A single injection of the isocratic test standard is made under the conditions given in Table 8: Table 8 Conditions Flow 1.
4 Using the Detector Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 9. The exact profile of the chromatogram will depend on the chromatographic conditions. Variations in solvent quality, column packing, standard concentration and column temperature will all have a potential effect on peak retention and response. Figure 9 Typical Chromatogram with UV-detector Optimization of the System The settings used for this analysis are specific for this purpose.
Using the Detector 4 Preparing the HPLC System 1 Turn on the Agilent ChemStation PC and the monitor. 2 Turn on the 1200 series HPLC modules. 3 Start the Agilent ChemStation software (B.02.01). If the pump, autosampler, thermostatted column compartment and detector are found, the ChemStation screen should look like shown in Figure 10. The System status is red (Not Ready).
4 Using the Detector 4 Turn on the detector lamp, pump and autosampler by clicking the System On button or the buttons below the module icons on the graphical user interface (GUI). After some time, the pump, thermostatted column compartment and detector module will turn to green.
Using the Detector 4 5 Purge the pump. For more information see “Priming and Purging the System" on page 40. 6 Allow the detector to warm up of at least 60 minutes to provide a stable baseline (see example in Figure 12). . NOTE For reproducible chromatography, the detector and lamp should be on for at least one hour. Otherwise the detector baseline may still drift (depending on the environment).
4 Using the Detector 7 For the isocratic pump, fill the solvent bottle with the mixture of HPLC-grade bi-distilled water (30 %) and acetonitrile (70 %). For binaryand quaternary pumps you can use separate bottles. 8 Click on the Load Method button and select DEF_LC.M and press OK. Alternative double-click on the method in the method window. The default LC method parameters are transferred into the 1200 modules.
Using the Detector 4 9 Click on the module icons (Figure 14) and open the Setup of these modules. Figure 15 on page 50 shows the detector settings (do not change the detector parameters at this time). Figure 14 Open the module menu 10 Enter the pump parameters mentioned under “Conditions" on page 43.
4 Using the Detector • 1 signal with individual wavelength setting • stop and post time can be set (if required) • peakwidth depends on the peaks in the chromatogram, see page 61. • time table for programmable actions during the run • Zero Offset Limits: 1 to 99% in steps of 1% • Attenuation Limits: 0.
Using the Detector 4 11 Pump the water/acetonitrile (30/70 %) mobile phase through the column for 10 minutes for equilibration. 12 Click the button and select Change... to open the Signal Plot information. Select the Pump: Pressure and the VWD A: Signal 254 as signals. Change the Y-range for the VWD to 1 mAU and the offset to 20% and the pressure offset to 50%. The X-axis range should be 15 minutes. Press OK to exit this screen.
4 Using the Detector The Online Plot (Figure 17 on page 52) shows both, the pump pressure and the detector absorbance signals. Pressing Adjust the signals can be reset to the offset value and Balance would do a balance on the detector. Pump pressure signal VWD absorbance signal Figure 17 Online Plot Window 13 If both baselines are stable, set the Y-range for the detector signal to 100 mAU.
Using the Detector 4 14 Select the menu item RunControl -> Sample Info and enter information about this application (Figure 18 on page 53). Press OK to leave this screen. Figure 18 Sample Information 15 Fill the content of an isocratic standard sample ampoule into a vial and seal the vial with a cap and place the vial into autosampler tray (position #1).
4 Using the Detector Running the Sample and Verifying the Results 1 To start a run select the menu item RunControl -> Run Method. 2 This will start the 1200 modules and the online plot on the Agilent ChemStation will show the resulting chromatogram. Figure 19 NOTE 54 Chromatogram with Isocratic Test Sample Information about using the Data Analysis functions can be obtained from the Using your ChemStation manual supplied with your system.
Using the Detector 4 Special Settings of the Detector In this chapter special settings of the G1314B VWD and G1314C VWD-SL are described (based on the Agilent ChemStation B.02.01). Control Settings • Lamp: turn on and off of UV-lamp. • At Power On: automatic lamp-on at power on. • Error Method: take error method or current method (in case of an error). • Analog Output Range: can be set to either 100 mV or 1 V full scale, see also “Analog Output Settings" on page 59.
4 Using the Detector Online Spectra 1 To view the online spectra select Online Spectra. NOTE This online spectrum is taken during a stop-flow condition only while the peak is kept in the flow cell, see “Scanning with the VWD" on page 57. Figure 21 Online Spectra Window 2 Change the absorbance and wavelength range according your needs.
Using the Detector 4 Scanning with the VWD NOTE Access to the scan feature is only possible during run. 1 Set up a run. 2 Start a run. 3 While running on the baseline, select from the menu Instrument - More VWD - Blank Scan, see Figure 22 on page 57. A background scan is stored in the memory. • Step 1: Blank Scan: scan of the background (solvent) is stored in the memory. • Step 2: Sample Scan: scan of the peak of interest is taken while the peak stays in the flow cell (stop-flow condition).
4 Using the Detector 5 Select from the menu Instrument - More VWD - Sample Scan. A sample scan is taken in the range defined under “Special Setpoints" on page 60 and the Online Spectra window (see “Online Spectra" on page 56) displays the result (Sample Scan minus Blank Scan).
Using the Detector 4 Analog Output Settings 1 To change the Output Range of the analog outputs select VWD Control. 2 To change the offset and the attenuation select VWD Signal - More. • Analog Output Range: can be set to either 100 mV or 1 V full scale. • Zero Offset: can be set to either 100 mV or 1 V full scale. • Attenuation Limits: 0.98 to 4000 mAU at discrete values for either 100 mV or 1 V full scale. Figure 23 Analog Output Settings 3 Change the values if required.
4 Using the Detector Special Setpoints 1 To change the offset and the attenuation select VWD Signal - More - Special Setpoints. Margin for negative Absorbance: Use this field to modify the detector’s signal handling to increase the margin for negative absorbance. Use this option if, for example, your solvent gradient produces a decreasing baseline absorbance, and for GPC analyses. Limits: 100 to 4000 mAU. Signal Polarity: can be switched to negative (if required).
Using the Detector 4 Peakwidth Settings NOTE Do not use peak width shorter than necessary, see also “Set the Detector Parameters" on page 69. 1 To change the Peakwidth settings select Setup Detector Signals. 2 In the section Peakwidth (Responsetime) click on the drop-down list. 3 Change the Peakwidth according to your needs. Peakwidth enables you to select the peak width (response time) for your analysis. The peak width is defined as the width of a peak, in minutes, at half the peak height.
4 Using the Detector Table 9 Peak Width (min) Response Time (sec) Data Rate (Hz) <0.005 0.12 13.74 >0.005 0.12 13.74 >0.01 0.25 13.74 >0.025 0.5 13.74 >0.05 1.0 6.87 >0.10 2.0 3.43 >0.20 4.0 1.72 >0.40 8.0 0.86 Table 10 62 Peak Width — Response Time — Data Rate (G1314B VWD) Peak Width — Response Time — Data Rate (G1314C VWD SL) Peak Width (min) Response Time (sec) Data Rate (Hz) <0.00125 <0.031 55 >0.00125 0.031 27.5 >0.0025 0.062 13.74 >0.005 0.12 13.74 >0.
Using the Detector 4 Optimizing the Detector Additional theoretical information can be found in chapter “How to optimize the detector" on page 65.
4 64 Using the Detector 1200 Series Variable Wavelength Detector User Manual
Agilent 1200 Series Variable Wavelength Detector User Manual 5 How to optimize the detector Optimizing the Detector Performance 66 This chapter gives hints on how to select the detector parameters and the flow cell.
5 How to optimize the detector Optimizing the Detector Performance The detector has a variety of parameters that can be used to optimize performance. The information below will guide you on how to get the best detector performance. Follow these rules as a start for new applications. It gives a rule-of-thumb for optimizing the detector parameters. Match the Flow Cell to the Column Figure 26 recommends the flow cell that matches the column used.
How to optimize the detector 5 Flow Cell Path Length Lambert-Beer’s law shows a linear relationship between the flow cell path length and absorbance.
5 How to optimize the detector Analysis of pesticide standard Absorbance 6-mm optical path length 10-mm optical path length Time (min) Figure 27 Influence of Cell Path Length on Signal Height Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards. To check photometric accuracy of the Agilent 1200 Series VWD it is necessary to have more precise information on path lengths of the VWD flow cells.
How to optimize the detector 5 Set the Detector Parameters 1 Set peakwidth as close as possible to the width (at half height) of a narrow peak of interest. Table 12 Peakwidth Settings Peakwidth at half height Rise time [10.. 90%] Data rate Module < 0.00125 minutes < 0.031 seconds 54.96 Hz G1314C 0.00125 minutes 0.031 seconds 27.48 Hz G1314C 0.0025 minutes 0.062 seconds 13.74 Hz G1314C 0.005 minutes 0.125 seconds 13.74 Hz G1314B / G1314C 0.01 minutes 0.25 seconds 13.
5 70 How to optimize the detector 1200 Series Variable Wavelength Detector User Manual
Agilent 1200 Series Variable Wavelength Detector User Manual 6 Troubleshooting and Diagnostics Overview of the Detector’s Indicators and Test Functions 72 Status Indicators 73 User Interfaces 75 Agilent LC Diagnostic Software 76 Overview about the troubleshooting and diagnostic features.
6 Troubleshooting and Diagnostics Overview of the Detector’s Indicators and Test Functions Status Indicators The detector is provided with two status indicators which indicate the operational state (prerun, run, and error states) of the detector. The status indicators provide a quick visual check of the operation of the detector (see page 51). Error Messages In the event of an electronic, mechanical or hydraulic failure, the detector generates an error message in the user interface.
Troubleshooting and Diagnostics 6 Status Indicators Two status indicators are located on the front of the detector. The lower left indicates the power supply status, the upper right indicates the detector status. Status indicator green/yellow/red Line power switch with green light Figure 28 Location of Status Indicators Power Supply Indicator The power supply indicator is integrated into the main power switch. When the indicator is illuminated (green) the power is ON.
6 Troubleshooting and Diagnostics Detector Status Indicator The detector status indicator indicates one of four possible detector conditions: • When the status indicator is OFF (and power switch light is on), the detector is in a prerun condition, and is ready to begin an analysis. • A green status indicator, indicates the detector is performing an analysis (run mode). • A yellow indicator indicates a not-ready condition.
Troubleshooting and Diagnostics 6 User Interfaces Depending on the user interface the available tests vary. All test descriptions are based on the Agilent ChemStation as user interface. Some descriptions are only available in the Service Manual. Table 13 NOTE Test Functions available vs.
6 Troubleshooting and Diagnostics Agilent LC Diagnostic Software The Agilent LC diagnostic software is an application independent tool that provides troubleshooting capabilities for the Agilent 1200 Series modules. It provides for all 1200 Series LC the possibility of a first guided diagnostic for typical HPLC symptoms and a status report stored as Adobe Acrobat pdf or as a printable file to assist users evaluating the instrument state.
Agilent 1200 Series Variable Wavelength Detector User Manual 7 Maintenance and Repair Introduction to Maintenance and Repair 78 Warnings and Cautions 79 Cleaning the Detector 80 Using the ESD Strap 81 This chapter provides general information on maintenance and repair of the detector.
7 Maintenance and Repair Introduction to Maintenance and Repair Simple Repairs - Maintenance The detector is designed for easy repair. The most frequent repairs such as lamp change and flow cell change can be done from the front of the detector with the detector in place in the system stack. These repairs are described in “Maintenance” on page 83 (part of the User Manual and Service Manual). Exchanging Internal Parts - Repair Some repairs may require exchange of defective internal parts.
Maintenance and Repair 7 Warnings and Cautions WA R N I N G To prevent personal injury, the power cable must be removed from the instrument before opening the detector cover. Do not connect the power cable to the detector while the covers are removed. WA R N I N G To prevent personal injury, be careful when getting in contact with sharp metal areas.
7 Maintenance and Repair Cleaning the Detector The detector case should be kept clean. Cleaning should be done with a soft cloth slightly dampened with water or a solution of water and mild detergent. Do not use an excessively damp cloth allowing liquid to drip into the detector. WA R N I N G 80 Do not let liquid drip into the detector. It could cause shock hazard and it could damage the detector.
Maintenance and Repair 7 Using the ESD Strap Electronic boards are sensitive to electrostatic discharge (ESD). In order to prevent damage, always use an ESD strap when handling electronic boards and components. 1 Unwrap the first two folds of the band and wrap the exposed adhesive side firmly around your wrist. 2 Unroll the rest of the band and peel the liner from the copper foil at the opposite end. 3 Attach the copper foil to a convenient and exposed electrical ground.
7 82 Maintenance and Repair 1200 Series Variable Wavelength Detector User Manual
Agilent 1200 Series Variable Wavelength Detector User Manual 8 Maintenance Overview of Maintenance 84 Exchanging a Lamp 85 Exchanging a Flow Cell 87 Repairing the Flow Cells 90 Using the Cuvette Holder 94 Correcting Leaks 97 Replacing Leak Handling System Parts 98 Replacing the Interface Board 99 Replacing the Detector’s Firmware 100 Tests & Calibrations 101 Intensity Test 102 Wavelength Verification/Calibration 104 Holmium Oxide Test 105 This chapter describes the maintenance of the detector.
8 Maintenance Overview of Maintenance The following pages describe maintenance (simple repairs) of the detector that can be carried out without opening the main cover. Table 14 Simple Repairs Procedures Typical Frequency Notes Deuterium lamp exchange If noise and/or drift exceeds your application limits or lamp does not ignite. A VWD test should be performed after replacement. Flow cell exchange If application requires a different flow cell type.
Maintenance 8 Exchanging a Lamp When required If noise or drift exceeds application limits or lamp does not ignite. Tools required Screwdriver POZI 1 PT3 Parts required Deuterium lamp G1314-60100 NOTE If you want to use the Agilent DAD lamp instead of the VWD lamp, you have to change the lamp settings in the VWD Configuration to lamp type 2140-0590. This ensures that the DAD lamp’s filament heating is operated like in the DAD. The instrument specifications are based on the VWD lamp.
8 Maintenance 4 Unscrew the lamp cover and remove it. 5 Unscrew, disconnect and replace the lamp. Insert, fix and reconnect the lamp. 6 Replace the lamp cover. 7 Replace the front cover. Next steps: • • • • 86 Reset the lamp counter as described in the User Interface documentation. Turn the lamp ON. Give the lamp more than 10 minutes to warm-up. Perform “Wavelength Verification/Calibration" on page 104 to check the correct positioning of the lamp.
Maintenance 8 Exchanging a Flow Cell When required If application needs a different type of flow cell or the flow cell needs repair.
8 Maintenance 2 Disconnect the inlet and outlet capillaries. 3 Unscrew the thumb screws parallel and remove the flow cell. Note: If you want to maintain flow cell parts, see “Repairing the Flow Cells" on page 90 or the information provided with your flow cell. 88 4 Replace the flow cell and fix the thumb screws. Reconnect the inlet and outlet capillaries to the flow cell.
Maintenance 5 Replace the front cover. 8 Next steps: • To check for leaks, establish a flow and observe the flow • • • 1200 Series Variable Wavelength Detector User Manual cell (outside of the cell compartment) and all capillary connections. Insert the flow cell. Perform “Wavelength Verification/Calibration" on page 104 to check the correct positioning of the flow cell. Replace the front cover.
8 Maintenance Repairing the Flow Cells NOTE When required If the flow cell needs repair due to leaks or contaminations. Tools required Wrench 1/4 inch for capillary connections Hexagonal wrench 4 mm Tooth picks Parts required See “Standard Flow Cell" on page 111. See “Micro Flow Cell" on page 112. See “Semi-micro Flow Cell" on page 113. See “High Pressure Flow Cell" on page 115. Preparations Turn off the flow. Remove the front cover. Remove the flow cell, see “Exchanging a Flow Cell" on page 87.
Maintenance Disassembling the Flow Cell 8 1 Unscrew the cell screw using a 4-mm hexagonal wrench. 2 Remove the SST rings using a pair of tweezers. 3 Use adhesive tape to remove the peek ring, the window and the gasket. CAUTION Do not use tweezers to remove windows as the surfaces can easily be scratched. 4 Repeat step 1 through step 3 for the other window (keep the parts separate - otherwise they could be mixed!).
8 Maintenance Next steps • Reconnect the capillaries, see “Exchanging a Flow Cell" on page 87. • Perform a leak test. If OK, insert the flow cell. • Perform “Wavelength Verification/Calibration" on page 104 to check the correct positioning of the flow cell. • Replace the front cover.
Maintenance 8 Using the Cuvette Holder When required: If your own standard should be used to checkout the instrument. Tools required: None Parts required: Cuvette Holder G1314-60200 Cuvette with the “standard”, e.g. NIST certified holmium oxide sample This cuvette holder can be placed instead of a flow cell in the variable wavelength detector. Standard cuvettes with standards in it, for example, National Institute of Standards & Technology (NIST) holmium oxide solution standard, can be fixed in it.
8 Maintenance Preparation for this procedure are: 1 Locate the cuvette holder on the desk. • Remove the normal flow cell. • Have cuvette with standard available. 2 Unscrew the bracket. 3 Insert the cuvette with the sample into the holder. The clear side of the cuvette must be visible. Light path Clear side Next steps: • • • • 94 Reset the lamp counter as described in the User Interface documentation. Turn the lamp ON. Give the lamp more than 10 minutes to warm-up.
Maintenance 4 Replace the bracket and fix the cuvette. 8 5 Install the cuvette holder in the instrument. Next steps: • Perform your verification.
8 Maintenance Correcting Leaks When required If a leakage has occurred in the flow cell area or at the capillary connections. Tools required Tissue Two 1/4 inch wrenches for capillary connections Parts required None 1 Remove the front cover. 2 Use tissue to dry the leak sensor area. 3 Observe the capillary connections and the flow cell area for leaks and correct, if required. 4 Replace the front cover.
Maintenance 8 Replacing Leak Handling System Parts When required If the parts are corroded or broken. Tools required None Parts required Leak funnel 5061-3356 Leak funnel holder 5041-8389 Leak tubing (120 mm) 0890-1711 1 Remove the front cover to have access to the leak handling system. 2 Pull the leak funnel out of the leak funnel holder. 3 Pull the leak funnel with the tubing out of its location. 4 Replace the leak funnel and/or the tubing.
8 Maintenance Replacing the Interface Board When required When defective or for installation of the board or for all repairs inside the detector. Part required Interface board (BCD) G1351-68701 with external contacts and BCD outputs. LAN Communication Interface board G1369A or G1369-60001. Tools required None 1 Install the ESD strap. Move the power lock across the power inlet. 2 If required, unscrew and remove the interface board. Place the board on the ESD kit.
Maintenance 8 Replacing the Detector’s Firmware When required If new version solves problems of currently installed version or after exchange of the detector main board (VWM) the version on board is older than previous installed one. Tools required LAN/RS-232 Firmware Update Tool, or Instant Pilot G4208A or Control Module G1323B Parts required Firmware, tools and documentation from Agilent web site Preparations Read update documentation provided with the Firmware Update Tool.
8 Maintenance Tests & Calibrations The following tests are required after maintenance of lamps and flow cells: • “Intensity Test" on page 102. • “Wavelength Verification/Calibration" on page 104. • “Holmium Oxide Test" on page 105.
Maintenance 8 Intensity Test The intensity test measures the intensity of the deuterium lamp over the full VWD wavelength range (190 – 600 nm). The test can be used to determine the performance of the lamp, and to check for dirty or contaminated flow cell windows. When the test is started, the gain is set to zero. To eliminate effects due to absorbing solvents, the test should be done with water in the flow cell.
8 Maintenance Figure 34 102 Intensity Test (Report) 1200 Series Variable Wavelength Detector User Manual
Maintenance 8 Wavelength Verification/Calibration Wavelength calibration of the detector is done using the zero-order position and 656 nm emission line position of the deuterium lamp. The calibration procedure involves two steps. First the grating is calibrated on the zero-order position. The stepper-motor step position where the zero-order maximum is detected is stored in the detector.
8 Maintenance Holmium Oxide Test This test verifies the calibration of the detector against the three wavelength maxima of the built-in holmium oxide filter. The test displays the difference between the expected and measured maxima. Figure 36 shows a holmium test spectrum. The test uses the following holmium maxima: • 360.8 nm • 418.5 nm • 536.4 nm NOTE See also “Declaration of Conformity for HOX2 Filter" on page 129.
Maintenance Figure 36 8 Holmium Test (Report) Holmium Oxide Test Failed Probable Causes • Detector not calibrated. • Dirty or defective flow cell. • Dirty or defective holmium oxide filter. • Optical misalignment.
8 Maintenance Suggested Actions ✔ Re-calibrate the detector. ✔ Repeat the test with the flow cell removed. If the test is OK, exchange the flow cell components. ✔ Run the holmium oxide filter test. If the test fails, exchange the filter assembly. ✔ Realign the optical components.
Maintenance 1200 Series Variable Wavelength Detector User Manual 8 107
8 108 Maintenance 1200 Series Variable Wavelength Detector User Manual
Agilent 1200 Series Variable Wavelength Detector User Manual 9 Parts and Materials for Maintenance Overview of Maintenance Parts 110 Standard Flow Cell 111 Micro Flow Cell 112 Semi-micro Flow Cell 113 High Pressure Flow Cell 115 Cuvette Holder 116 Leak Parts 117 Accessory Kit 118 This chapter provides information on parts for maintenance.
9 Parts and Materials for Maintenance Overview of Maintenance Parts Table 15 Item 110 Maintenance Parts Description Part Number Cable CAN assembly 0.
Parts and Materials for Maintenance 9 Standard Flow Cell Table 16 Item Standard Flow Cell Assembly Description Part Number Standard Flow Cell, 10 mm, 14 µl, 40 bar G1314-60086 1 Cell screw kit, quantity=2 G1314-65062 2 Conical spring kit, quantity=10 79853-29100 3 Ring #1 PEEK kit, quantity=2 G1314-65065 4 Gasket #1 (small hole), KAPTON, quantity=10 G1314-65063 5 Window quartz kit, quantity=2 79853-68742 6 Gasket #2 (large hole), KAPTON, quantity=10 G1314-65064 7 Ring #2 PEEK kit
9 Parts and Materials for Maintenance Micro Flow Cell Table 17 Item Description Part Number Micro flow cell, 5 mm, 1 µl, 40 bar G1314-60081 Capillary column – detector SST 400 mm lg, 0.12 i.d.
Parts and Materials for Maintenance 9 Semi-micro Flow Cell Table 18 Item Description Part Number Semi-micro flow cell assembly, 6 mm, 5 µl, 40 bar G1314-60083 Cell screw 79853-27200 Semi-micro cell kit, consisting of: two windows, two #1 standard gaskets, one #1 semi-micro gasket and one #2 semi-micro gasket.
9 Parts and Materials for Maintenance 1 - Cell screw 2 - Conical springs 3 - Ring SST 4 - Gasket #1 5 - Quartz window 6 - Semi-micro gasket #1 7 - Semi-micro gasket #2 1 2 3 4 5 7 6 5 4 3 2 1 Figure 39 114 Semi-micro Flow Cell 1200 Series Variable Wavelength Detector User Manual
Parts and Materials for Maintenance 9 High Pressure Flow Cell Table 19 Item High Pressure Flow Cell Assembly Description Part Number High pressure flow cell, 10 mm, 14 µl, 400 bar G1314-60082 Capillary column–detector SST 380 mm lg, 0.17 i.d.
9 Parts and Materials for Maintenance Cuvette Holder Table 20 Item Cuvette Holder Description Part Number Cuvette Holder G1314-60200 For information the use of the cuvette holder, refer to “Using the Cuvette Holder" on page 94.
Parts and Materials for Maintenance 9 Leak Parts Table 21 Leak Parts Item Description Part Number 3 Leak funnel 5041-8388 4 Leak funnel holder 5041-8389 5 Clip 5041-8387 6 Corrugated tubing, 120 mm lg, re-order 5 m 5062-2463 7 Corrugated tubing, 1200 mm lg, re-order 5 m 5062-2463 5 4 3 6 7 Figure 42 Leak Parts 1200 Series Variable Wavelength Detector User Manual 117
9 Parts and Materials for Maintenance Accessory Kit This kit contains some accessories and tools needed for the installation and repair of the detector. Table 22 118 Accessory Kit Parts Description Part Number Accessory kit G1314-68705 Corrugated tubing (to waste), re-order 5 m 5062-2463 Peek outlet capillary kit, i.d. is 0.25 mm (PEEK) 5062-8535 Fitting male PEEK, quantity=1 0100-1516 Hex key 1.
Agilent 1200 Series Variable Wavelength Detector User Manual A Appendix General Safety Information 120 Lithium Batteries Information 123 Radio Interference 124 Sound Emission 125 UV-Radiation 126 Solvent Information 127 Declaration of Conformity for HOX2 Filter 129 Agilent Technologies on Internet 130 This chapter provides addition information on safety, legal and web.
A Appendix General Safety Information The following general safety precautions must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Agilent Technologies assumes no liability for the customer’s failure to comply with these requirements.
Appendix CAUTION A The operator of this instrument is advised that if the equipment is used in a manner not specified in this manual, the protection provided by the equipment may be impaired. Some adjustments described in the manual, are made with power supplied to the instrument, and protective covers removed. Energy available at many points may, if contacted, result in personal injury. Any adjustment, maintenance, and repair of the opened instrument under voltage should be avoided as much as possible.
A Appendix Safety Symbols Table 23 shows safety symbols used on the instrument and in the manuals. Table 23 Symbol ! Safety Symbols Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect the apparatus against damage. Indicates dangerous voltages. Indicates a protected ground terminal. Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product.
Appendix A Lithium Batteries Information WA R N I N G Danger of explosion if battery is incorrectly replaced. Replace only with the same or equivalent type recommended by the equipment manufacturer. Lithium batteries may not be disposed-off into the domestic waste. Transportation of discharged Lithium batteries through carriers regulated by IATA/ICAO, ADR, RID, IMDG is not allowed. Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries.
A Appendix Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations. Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and/or used for measurements on open set-ups, the user has to assure that under operating conditions the radio interference limits are still met within the premises.
Appendix A Sound Emission Manufacturer’s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991. This product has a sound pressure emission (at the operator position) < 70 dB.
A Appendix UV-Radiation Emissions of ultraviolet radiation (200-315 nm) from this product is limited such that radiant exposure incident upon the unprotected skin or eye of operator or service personnel is limited to the following TLVs (Threshold Limit Values) according to the American Conference of Governmental Industrial Hygienists: Table 24 UV-Radiation Limits Exposure/day Effective Irradiance 8 hours 0.1 µW/cm2 10 minutes 5.
Appendix A Solvent Information Observe the following recommendations on the use of solvents. Flow Cell Avoid the use of alkaline solutions (pH > 9.5) which can attack quartz and thus impair the optical properties of the flow cell. Prevent any crystallization of buffer solutions. This will lead into a blockage/damage of the flow cell. If the flow cell is transported while temperatures are below 5 degree C, it must be assured that the cell is filled with alcohol.
A Appendix • Chromatographic grade ethers, which can contain peroxides (for example, THF, dioxane, di-isopropylether) such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides. • Solutions of organic acids (acetic acid, formic acid, and so on) in organic solvents. For example, a 1-% solution of acetic acid in methanol will attack steel. • Solutions containing strong complexing agents (for example, EDTA, ethylene diamine tetra-acetic acid).
Appendix A Declaration of Conformity for HOX2 Filter 1200 Series Variable Wavelength Detector User Manual 129
A Appendix Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at: http://www.agilent.com Select “Products” - “Chemical Analysis” It will provide also the latest firmware of the Agilent 1200 Series modules for download.
Index Index A absorbance Beer-Lambert, 67 accessory kit (parts), 118 Agilent ChemStation, 45 LC diagnostic software, 76 on internet, 130 Agilent on internet, 130 algea information, 127 analog output range, 55, 59 output settings, 59 ASTM environmental conditions, 23 reference and conditions, 26 attenuation, 50 autobalance, 50 automatic turn on, 55 B band width 6.
Index leak correcting, 97 panels (parts), 117 line power consumption, 24 voltage and frequency, 24 linearity, 25, 26 M maintenance, 83 cleaning the instrument, 80 correcting leaks, 97 exchanging flow cell, 87 exchanging interface board, 99 exchanging lamps, 85 exchanging leak handling system, 98 for parts see ’parts for maintenance’, 109 introduction, 77 overview, 84 replacing firmware, 100 simple repairs, 78 standard flow cell, 90 using the cuvette holder, 94 using the ESD strap, 81 method error, 55 load
Index special settings, 55 specifications performance, 25 physical, 24 spectra online, 56 stable baseline, 47 stack configuration, 30, 32 rear view, 32 standards, 24 status indicators, 72, 74 stop time, post time, 50 stop-flow condition, 56 T test functions, 72 tests holmium oxide, holmium oxide test, 105 intensity of lamp, 102 wavelength calibration, 104 time table, 50 troubleshooting Agilent LC diagnostic software, 76 diagnostic signals, 72 error messages, 72 overview, 72 status indicator, 74 status ind
Index 134 1200 Series Variable Wavelength Detector User Manual
www.agilent.com In This Book This manual contains the technical reference information about the Agilent 1200 Series variable wavelength detector. The manual describes the following: • introcduction and specifications, • installation, • using and optimizing, • troubleshooting overview, • maintenance, • parts identification, • safety and related information.
